EP3233748B1 - Sonnenschutzverglasung oder verglasung mit geringer emissivität mit einer oberen schutzschicht - Google Patents
Sonnenschutzverglasung oder verglasung mit geringer emissivität mit einer oberen schutzschicht Download PDFInfo
- Publication number
- EP3233748B1 EP3233748B1 EP15823645.5A EP15823645A EP3233748B1 EP 3233748 B1 EP3233748 B1 EP 3233748B1 EP 15823645 A EP15823645 A EP 15823645A EP 3233748 B1 EP3233748 B1 EP 3233748B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- layer
- silver
- stack
- metal layer
- functional metal
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 239000011241 protective layer Substances 0.000 title claims description 19
- 239000010410 layer Substances 0.000 claims description 136
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 49
- 239000000758 substrate Substances 0.000 claims description 44
- 229910052709 silver Inorganic materials 0.000 claims description 42
- 239000004332 silver Substances 0.000 claims description 42
- 239000000463 material Substances 0.000 claims description 37
- 229910052751 metal Inorganic materials 0.000 claims description 29
- 239000002184 metal Substances 0.000 claims description 29
- 239000010936 titanium Substances 0.000 claims description 29
- 238000000576 coating method Methods 0.000 claims description 22
- 230000000903 blocking effect Effects 0.000 claims description 21
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 19
- 238000010438 heat treatment Methods 0.000 claims description 18
- 239000011248 coating agent Substances 0.000 claims description 14
- 229910052719 titanium Inorganic materials 0.000 claims description 14
- 229910052710 silicon Inorganic materials 0.000 claims description 13
- 239000010703 silicon Substances 0.000 claims description 13
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims description 11
- 229910052726 zirconium Inorganic materials 0.000 claims description 11
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 10
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
- 239000011651 chromium Substances 0.000 claims description 6
- 239000010955 niobium Substances 0.000 claims description 6
- 238000004544 sputter deposition Methods 0.000 claims description 6
- 150000002739 metals Chemical class 0.000 claims description 5
- 229910052758 niobium Inorganic materials 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 4
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 3
- 239000011521 glass Substances 0.000 claims description 3
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims description 3
- 229910052715 tantalum Inorganic materials 0.000 claims description 3
- 229910045601 alloy Inorganic materials 0.000 claims description 2
- 239000000956 alloy Substances 0.000 claims description 2
- 229910052804 chromium Inorganic materials 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- 239000005361 soda-lime glass Substances 0.000 claims description 2
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims description 2
- 230000001747 exhibiting effect Effects 0.000 claims 2
- ZARVOZCHNMQIBL-UHFFFAOYSA-N oxygen(2-) titanium(4+) zirconium(4+) Chemical compound [O-2].[O-2].[O-2].[O-2].[Ti+4].[Zr+4] ZARVOZCHNMQIBL-UHFFFAOYSA-N 0.000 claims 2
- QERYCTSHXKAMIS-UHFFFAOYSA-M thiophene-2-carboxylate Chemical compound [O-]C(=O)C1=CC=CS1 QERYCTSHXKAMIS-UHFFFAOYSA-M 0.000 claims 1
- 238000012360 testing method Methods 0.000 description 31
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 11
- 230000007797 corrosion Effects 0.000 description 11
- 238000005260 corrosion Methods 0.000 description 11
- 238000003860 storage Methods 0.000 description 8
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 8
- 238000010791 quenching Methods 0.000 description 7
- 230000000171 quenching effect Effects 0.000 description 7
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 6
- 229910052782 aluminium Inorganic materials 0.000 description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 6
- 230000005540 biological transmission Effects 0.000 description 6
- 230000007547 defect Effects 0.000 description 6
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 6
- 230000000087 stabilizing effect Effects 0.000 description 6
- 229910001928 zirconium oxide Inorganic materials 0.000 description 6
- 230000004888 barrier function Effects 0.000 description 5
- 239000002346 layers by function Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 239000011135 tin Substances 0.000 description 5
- 229910052718 tin Inorganic materials 0.000 description 5
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 4
- 238000000137 annealing Methods 0.000 description 4
- 230000003287 optical effect Effects 0.000 description 4
- 229910052581 Si3N4 Inorganic materials 0.000 description 3
- 241001080024 Telles Species 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 3
- 239000004411 aluminium Substances 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 3
- 239000003086 colorant Substances 0.000 description 3
- 238000000151 deposition Methods 0.000 description 3
- 150000004767 nitrides Chemical class 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 3
- 238000011282 treatment Methods 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 239000011787 zinc oxide Substances 0.000 description 3
- 229910003087 TiOx Inorganic materials 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 238000005452 bending Methods 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 239000000428 dust Substances 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 230000014509 gene expression Effects 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 241000894007 species Species 0.000 description 2
- HLLICFJUWSZHRJ-UHFFFAOYSA-N tioxidazole Chemical compound CCCOC1=CC=C2N=C(NC(=O)OC)SC2=C1 HLLICFJUWSZHRJ-UHFFFAOYSA-N 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- 229910000599 Cr alloy Inorganic materials 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 229910000990 Ni alloy Inorganic materials 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- 239000012080 ambient air Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000013626 chemical specie Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000005224 laser annealing Methods 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 229910000484 niobium oxide Inorganic materials 0.000 description 1
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910001936 tantalum oxide Inorganic materials 0.000 description 1
- 238000005496 tempering Methods 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
- C03C17/36—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal
- C03C17/3602—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer
- C03C17/3657—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer the multilayer coating having optical properties
- C03C17/366—Low-emissivity or solar control coatings
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
- C03C17/36—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
- C03C17/36—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal
- C03C17/3602—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer
- C03C17/3615—Coatings of the type glass/metal/other inorganic layers, at least one layer being non-metallic
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
- C03C17/36—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal
- C03C17/3602—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer
- C03C17/3644—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer the metal being silver
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/20—Materials for coating a single layer on glass
- C03C2217/21—Oxides
- C03C2217/212—TiO2
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/20—Materials for coating a single layer on glass
- C03C2217/21—Oxides
- C03C2217/23—Mixtures
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/20—Materials for coating a single layer on glass
- C03C2217/25—Metals
- C03C2217/251—Al, Cu, Mg or noble metals
- C03C2217/254—Noble metals
- C03C2217/256—Ag
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/20—Materials for coating a single layer on glass
- C03C2217/28—Other inorganic materials
- C03C2217/281—Nitrides
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/70—Properties of coatings
- C03C2217/78—Coatings specially designed to be durable, e.g. scratch-resistant
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2218/00—Methods for coating glass
- C03C2218/10—Deposition methods
- C03C2218/15—Deposition methods from the vapour phase
- C03C2218/154—Deposition methods from the vapour phase by sputtering
- C03C2218/156—Deposition methods from the vapour phase by sputtering by magnetron sputtering
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2218/00—Methods for coating glass
- C03C2218/30—Aspects of methods for coating glass not covered above
- C03C2218/32—After-treatment
Definitions
- the invention relates to a material and a method for obtaining a material, such as glazing, comprising a transparent substrate coated with a stack of thin layers comprising at least one functional metallic layer based on silver.
- Materials comprising functional silver-based metallic layers (or silver layers) are used in so-called “solar control” glazing aimed at reducing the amount of incoming solar energy and / or in so-called “low-emissive” glazing. »Aiming to reduce the amount of energy dissipated to the outside of a building or a vehicle by virtue of their advantageous properties of electrical conduction and reflection of infrared (IR) radiation.
- IR infrared
- coated substrates are generally not strong enough to be used in applications where the stack is directly in contact with an uncontrolled medium such as ambient air in the case of single glazing.
- these substrates can be used in the form of multiple, double or triple glazing.
- the stack is then positioned inside the multiple glazing, in contact with a sealed medium consisting of the gas from the intermediate blade. The stack is thus protected from humidity and dust.
- the coated substrate of the stack can be stepped. This consists in removing at the periphery of the substrate, over an area of at least 1 mm in width, one or more thin layers so that they do not reach the edges of the substrate and thus avoid corrosion phenomena.
- the coated substrates undergo before assembly various processing steps such as cutting, washing, edge shaping and / or heat treatments at high temperature such as quenching, annealing and / or bending. It is common and practical to carry out the assembly and / or the various treatments at a location other than that where the substrate coated with the stack is manufactured. These substrates therefore also undergo stages of storage and transport under variable climatic conditions.
- the substrates coated with the stacks are subjected, during these different steps, to mechanical and chemical stresses resulting from very different conditions defined in particular by the temperature, humidity and the nature of the species constituting the medium in contact with the stack.
- the main factors liable to deteriorate the stacks during a heat treatment at high temperature are different from the factors intervening during the normal use of the substrate for its dedicated application or during storage. During a treatment at high temperature, these factors are the temperature in general above 400 ° C., the pressure and the nature of the chemical species liable to be in contact with the stack. During normal use or storage, these factors are the desired shelf life or shelf life, the characteristics of the medium in contact with the stack such as humidity, the temperature generally below 100 ° C and the presence possible dust.
- These upper protective layers are deposited in the form of a metal or a metal oxide chosen from at least one of the following metals: Nb, Sn, Ta, Ti, Zr or of the following oxides: niobium oxide, d oxide tin, tantalum oxide, titanium oxide, zirconium oxide.
- these metals in particular niobium, tin and titanium, have the common point of forming, by oxidizing, a compound with sodium so as to limit its diffusion into the underlying layers.
- the titanium oxide-based layers make it possible to obtain effective protection of the stack following a heat treatment at high temperature as well as good mechanical strength.
- the substrates coated with such protective layers are subject to cold corrosion in a humid environment when the stack is not trapped in double glazing and during the various stages of storage and / or processing.
- WO 2014/191472 discloses a low emissivity stack coated substrate.
- the applicant has surprisingly discovered that the use as an upper protective layer of a layer of titanium and zirconium oxide having a particular titanium to zirconium weight ratio makes it possible to achieve these objectives by considerably improving the resistance to cold corrosion while retaining good resistance to heat treatment at high temperature and good mechanical strength.
- the invention relates to a material according to claim 1.
- the upper protective layer based on titanium and zirconium oxide has, in increasing order of preference, a ratio by weight of titanium to zirconium Ti / Zr of between 60/40 and 80/20, between 60/40 and 70 / 30, between 60/40 and 65/35 or between 60/40 and 64/36.
- the upper protective layer based on titanium and zirconium oxide has, in increasing order of preference, an atomic ratio of titanium to zirconium Ti / Zr of between 70/30 and 95/5, between 70/30 and 85/15, between 70/30 and 80/20.
- the layers of titanium and zirconium oxide can be deposited from a ceramic target of TiZrOx.
- the ratio of titanium to zirconium Ti / Zr in the layer is almost equivalent to that of the target.
- the ceramic targets can optionally comprise other elements which are found in the layers deposited from these targets.
- the upper protective layer is preferably the last layer of the stack, that is to say the layer furthest from the substrate coated with the stack.
- the dielectric layer based on silicon and / or aluminum nitride is in contact with the upper protective layer based on titanium and zirconium oxide.
- the silver layers are deposited between dielectric coatings which generally comprise several dielectric layers making it possible to adjust the optical properties of the stack. These dielectric layers also make it possible to protect the silver layer from chemical or mechanical attack.
- the stack of thin layers therefore advantageously comprises at least one functional metal layer based on silver, at least two dielectric coatings, each dielectric coating comprising at least one dielectric layer, so that each functional metal layer is placed between two dielectric coatings.
- the stack of thin layers comprises a single functional layer.
- the stack is deposited by cathodic sputtering, in particular assisted by a magnetic field (magnetron process). According to this advantageous embodiment, all the layers of the stack are deposited by cathodic sputtering assisted by a magnetic field.
- thicknesses mentioned in this document are physical thicknesses.
- the term “thin layer” is understood to mean a layer having a thickness of between 0.1 nm and 100 micrometers.
- the substrate according to the invention is considered to be laid horizontally.
- the stack of thin layers is deposited above the substrate.
- the meaning of the expressions “above” and “below” and “lower” and “upper” is to be considered in relation to this orientation.
- the expressions “above” and “below” do not necessarily mean that two layers and / or coatings are disposed in contact with each other. When it is specified that a layer is deposited “in contact” with another layer or with a coating, this means that there cannot be one or more layers interposed between these two layers.
- the functional silver-based metallic layer comprises at least 95.0%, preferably at least 96.5% and better still at least 98.0% by weight of silver relative to the weight of the functional layer.
- the silver-based functional metal layer comprises less than 1.0% by weight of metals other than silver based on the weight of the silver-based functional metal layer.
- the thickness of the functional silver-based layers is, in increasing order of preference, from 5 to 20 nm, from 8 to 15 nm.
- the stack may comprise at least one blocking layer, the function of which is to protect the silver layers by preventing possible degradation linked to the deposition of a dielectric coating or linked to a heat treatment.
- These blocking layers are preferably located in contact with the functional silver-based metal layers.
- the stack may comprise at least one blocking layer located below and in contact with a functional metallic layer based on silver and / or at least one blocking layer located above and in contact with a functional metallic layer based on silver.
- blocking layers based on a metal chosen from niobium Nb, tantalum Ta, titanium Ti, chromium Cr or nickel Ni or based on an alloy obtained. from at least two of these metals, in particular an alloy of nickel and chromium (NiCr).
- the dielectric coatings have a thickness greater than 15 nm, preferably between 15 and 50 nm and better still from 30 to 40 nm.
- dielectric layers with a barrier function is understood to mean a layer made of a material capable of forming a barrier to the diffusion of oxygen and water at high temperature, originating from the ambient atmosphere or from the transparent substrate, towards the functional layer.
- the dielectric layers with a barrier function may be based on silicon and / or aluminum compounds chosen from oxides such as SiO 2 , nitrides such as silicon nitride Si 3 N 4 and aluminum nitrides AIN, and SiO x N y oxynitrides, optionally doped with at least one other element.
- the dielectric layers with a barrier function can also be based on zinc oxide and tin.
- dielectric layers with a stabilizing function is understood to mean a layer made of a material capable of stabilizing the interface between the functional layer and this layer.
- the dielectric layers with a stabilizing function are preferably based on crystalline oxide, in particular based on zinc oxide, optionally doped with at least one other element, such as aluminum.
- the dielectric layer (s) with a stabilizing function are preferably layers of zinc oxide.
- the dielectric layer (s) with a stabilizing function may be located above and / or below at least one functional metallic layer based on silver or each functional metallic layer based on silver, either directly in contact with it. or either separated by a blocking layer.
- the transparent substrates according to the invention are preferably made of a rigid mineral material, such as glass, in particular soda-lime-silica.
- the thickness of the substrate generally varies between 0.5 mm and 19 mm.
- the thickness of the substrate is preferably less than or equal to 6 mm, or even 4 mm.
- the material that is to say the transparent substrate coated with the stack, may be intended to undergo a heat treatment at high temperature chosen from an annealing, for example by a flash annealing such as a laser annealing or flaming, quenching and / or bending.
- the temperature of the heat treatment is greater than 400 ° C, preferably greater than 450 ° C, and better still greater than 500 ° C.
- the substrate coated with the stack can therefore be bent and / or tempered.
- the material may be in the form of monolithic glazing, laminated glazing or multiple glazing, in particular double glazing or triple glazing.
- the material of the invention is suitable in all applications requiring the use of a stack comprising layers of silver for which the resistance to heat treatment and to cold corrosion are key parameters such as low-emissive glazing for buildings. , glazing for refrigerator door.
- the invention also relates to a method according to claim 13.
- the method may further comprise the step during which the substrate coated with the stack of thin layers is subjected to a heat treatment at a temperature above 400 ° C, preferably 500 ° C.
- Stacks of thin layers defined below are deposited on clear soda-lime glass substrates with a thickness of 4 mm.
- Magnetic cathode sputtering the conditions for depositing the layers deposited by sputtering (so-called “magnetron cathode sputtering”) are summarized in Table 1 below.
- the layers of titanium oxide and zirconium are deposited from a ceramic target of TiZrOx.
- the titanium to zirconium Ti / Zr ratio in the target is 64:36 by weight corresponding to 77:23 atomic.
- the ratio of titanium to zirconium Ti / Zr in the layer is almost equivalent to that of the target.
- the substrates coated with protected stacks according to the invention are hardenable, bent and do not need to be edged when they are mounted in double glazing.
- Glazing Comparative Invention Top layer of protection TiZrOx - 3 TiOx 3 - Dielectric coating If 3 N 4 35 35 OB blocking layer NiCr 0.4 0.4 Functional layer Ag 7 7 UB blocking layer NiCr 0.7 0.7 Dielectric coating If 3 N 4 35 35 Substrate (mm) glass 4 4 4
- HH High Humidity
- CV Cleveland
- the high humidity test (HH) consists of storing samples at 95% relative humidity and at 40 ° C and observing the possible presence of defects such as pitting corrosion.
- the materials comprising the protective layer according to the invention withstand the two tests for at least 56 days while the comparative material exhibits defects from 7 days to the HH test and from 26 days to the CV test.
- the solution of the invention makes it possible to significantly improve the life of the material, in particular by a factor of 2 or 8 according to the HH or CV test.
- the Erichsen Brush test (EBT) consists of subjecting different coated substrates before (EBT) and after tempering (TT-EBT) to a certain number of cycles (1000) during which the stack covered with water is rubbed with water. using a brush. A substrate is considered to pass the test if no mark is visible to the naked eye.
- the test before toughening gives a good indication of the ability of the glazing to be scratched during a washing operation.
- the test after quenching gives a good indication of the propagation of scratches after heat treatment.
- the Opel test evaluates abrasion resistance. It is carried out in accordance with standard EN1096-2 at 2000 cycles.
- the cleaning test consists of three washing machine passes of the substrate.
- the material according to the invention satisfies each of its tests.
- the material according to the invention protected with an upper protective layer of TiZrOx was heated for 500 h at 400 ° C. No degradation is observed.
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Surface Treatment Of Glass (AREA)
- Laminated Bodies (AREA)
Claims (14)
- Material, umfassend ein mit einer Stapelung dünner Schichten, umfassend mindestens eine metallische Funktionsschicht auf Basis von Silber, beschichtetes transparentes Substrat, dadurch gekennzeichnet, dass die Stapelung Folgendes umfasst:- eine dielektrische Schicht auf Basis von Siliciumnitrid und/oder von Aluminium mit einer Dicke von mindestens 25 nm, die sich über einer metallischen Funktionsschicht auf Basis von Silber befindet,- eine obere Schutzschicht auf Basis von Titan- und Zirconiumoxid, die sich über und in Kontakt mit der dielektrischen Schicht auf Basis von Siliciumnitrid und/oder von Aluminium befindet, die ein Gewichtsverhältnis von Titan zu Zirconium Ti/Zr im Bereich zwischen 60:40 und 80:20 aufweist unddadurch gekennzeichnet, dass die Gesamtdicke aller in der Stapelung vorhandenen Oxidschichten kleiner als 10 nm ist.
- Material nach Anspruch 1, dadurch gekennzeichnet, dass die obere Schutzschicht eine Dicke aufweist:- von höchstens 5 nm und/oder- von mindestens 2 nm.
- Material nach Anspruch 1 oder 2, dadurch gekennzeichnet, dass die dielektrische Schicht auf Basis von Siliciumnitrid und/oder Aluminium eine Dicke von höchstens 50 nm aufweist.
- Material nach einem der vorstehenden Ansprüche, dadurch gekennzeichnet, dass das Gewichtsverhältnis von Titan zu Zirconium Ti/Zr im Bereich zwischen 60:40 und 70:30 liegt.
- Material nach einem der vorstehenden Ansprüche, dadurch gekennzeichnet, dass die Stapelung von dünnen Schichten mindestens eine metallische Funktionsschicht auf Basis von Silber, mindestens zwei dielektrische Beschichtungen umfasst, wobei jede dielektrische Beschichtung mindestens eine dielektrische Schicht umfasst, sodass jede metallische Funktionsschicht zwischen zwei dielektrischen Beschichtungen angeordnet ist.
- Material nach einem der vorstehenden Ansprüche, dadurch gekennzeichnet, dass die Stapelung mindestens eine Blockierschicht umfasst, die sich unter und in Kontakt mit einer metallischen Funktionsschicht auf Basis von Silber befindet.
- Material nach einem der vorstehenden Ansprüche, dadurch gekennzeichnet, dass die Stapelung mindestens eine Blockierschicht umfasst, die sich über und in Kontakt mit einer metallischen Funktionsschicht auf Basis von Silber befindet.
- Material nach einem der Ansprüche 6 bis 7, dadurch gekennzeichnet, dass die Blockierschichten auf einem Metall basieren, das aus Niob Nb, Tantal Ta, Titan Ti, Chrom Cr oder Nickel Ni oder einer Legierung ausgewählt ist, die ausgehend von mindestens zwei dieser Metalle erhalten wird.
- Material nach einem der vorstehenden Ansprüche, dadurch gekennzeichnet, dass die Stapelung Folgendes umfasst:- eine dielektrische Beschichtung, die sich unter der metallischen Funktionsschicht auf Basis von Silber befindet,- gegebenenfalls eine Blockierschicht,- eine metallische Funktionsschicht auf Basis von Silber,- gegebenenfalls eine Blockierschicht,- eine dielektrische Beschichtung, die sich über der metallischen Funktionsschicht auf Basis von Silber befindet,- eine obere Schutzschicht.
- Material nach einem der vorstehenden Ansprüche, dadurch gekennzeichnet, dass die Stapelung Folgendes umfasst:- eine dielektrische Beschichtung, die sich unter der metallischen Funktionsschicht auf Basis von Silber befindet, umfassend mindestens eine dielektrische Schicht auf Basis von Siliciumnitrid und/oder Aluminium,- gegebenenfalls eine Blockierschicht,- eine metallische Funktionsschicht auf Basis von Silber,- gegebenenfalls eine Blockierschicht,- eine dielektrische Beschichtung, die sich über der metallischen Funktionsschicht auf Basis von Silber befindet, umfassend mindestens eine dielektrische Schicht auf Basis von Siliciumnitrid und/oder Aluminium,- eine obere Schutzschicht.
- Material nach einem der vorstehenden Ansprüche, wobei das Substrat aus Glas wie beispielsweise aus Kalknatronsilikatglas, besteht.
- Material nach einem der vorstehenden Ansprüche, dadurch gekennzeichnet, dass mindestens das beschichtete Substrat der Stapelung gebogen und/oder gehärtet ist.
- Verfahren zum Erhalten eines Materials, umfassend ein mit einer Stapelung aus dünnen Schichten, die durch Kathodenzerstäubung, gegebenenfalls durch Magnetfeld unterstützt, abgeschieden werden, beschichtetes transparentes Substrat, wobei das Verfahren die Abfolge der folgenden Schritte umfasst:- Auftragen mindestens einer metallischen Funktionsschicht auf Basis von Silber auf das Substrat, danach- Auftragen mindestens einer dielektrischen Schicht auf Basis von Siliciumnitrid und/oder von Aluminium mit einer Dicke von mindestens 25 nm über die metallische Funktionsschicht auf Basis von Silber,- Auftragen einer oberen Schutzschicht auf Basis von Titan- und Zirconiumoxid, die ein Gewichtsverhältnis von Titan zu Zirconium Ti/Zr im Bereich zwischen 60:40 und 80:20 aufweist, über und in Kontakt mit der dielektrischen Schicht auf Basis von Siliciumnitrid und/oder Aluminium unddadurch gekennzeichnet, dass die Gesamtdicke aller in der Stapelung vorhandenen Oxidschichten kleiner als 10 nm ist.
- Verfahren nach Anspruch 13, wobei dies des Weiteren den Schritt umfasst, während welchem das mit der Stapelung dünner Schichten beschichtete Substrat einer thermischen Behandlung bei einer Temperatur von höher als 400 °C unterzogen wird.
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PL15823645T PL3233748T3 (pl) | 2014-12-19 | 2015-12-14 | Szyba regulująca nasłonecznienie lub niskoemisyjna zawierająca wierzchnią warstwę ochronną |
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FR1462871A FR3030494B1 (fr) | 2014-12-19 | 2014-12-19 | Vitrage de controle solaire ou bas emissif comprenant une couche de protection superieure |
PCT/FR2015/053473 WO2016097557A1 (fr) | 2014-12-19 | 2015-12-14 | Vitrage contrôle solaire ou bas émissif comprenant une couche de protection supérieure |
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EP3233748A1 EP3233748A1 (de) | 2017-10-25 |
EP3233748B1 true EP3233748B1 (de) | 2020-11-25 |
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EP15823645.5A Active EP3233748B1 (de) | 2014-12-19 | 2015-12-14 | Sonnenschutzverglasung oder verglasung mit geringer emissivität mit einer oberen schutzschicht |
Country Status (10)
Country | Link |
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US (1) | US20170355639A1 (de) |
EP (1) | EP3233748B1 (de) |
KR (1) | KR102523455B1 (de) |
BR (1) | BR112017012191B1 (de) |
CO (1) | CO2017005826A2 (de) |
ES (1) | ES2836351T3 (de) |
FR (1) | FR3030494B1 (de) |
MX (1) | MX2017007942A (de) |
PL (1) | PL3233748T3 (de) |
WO (1) | WO2016097557A1 (de) |
Families Citing this family (7)
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EP3680437B1 (de) * | 2017-09-08 | 2023-10-04 | LG Hausys, Ltd. | Funktionsbaustoff für tür und fenster |
KR102655096B1 (ko) * | 2019-04-26 | 2024-04-04 | 쌩-고벵 글래스 프랑스 | 코팅 물품 및 이의 제조 방법 |
FR3101344A1 (fr) | 2019-09-30 | 2021-04-02 | Saint-Gobain Glass France | Vitrage comprenant un empilement antisolaire et un revêtement protecteur comprenant de l’yttrium |
KR20210050042A (ko) * | 2019-10-25 | 2021-05-07 | 쌩-고벵 글래스 프랑스 | 박막 다층 코팅이 구비된 투명 기재 및 이를 포함하는 다중 글레이징 유닛 |
KR20210074757A (ko) * | 2019-12-12 | 2021-06-22 | 쌩-고벵 글래스 프랑스 | 박막 다층 코팅이 구비된 투명 기재 |
FR3129938A1 (fr) | 2021-12-08 | 2023-06-09 | Saint-Gobain Glass France | Vitrage comprenant un empilement antisolaire et un revêtement protecteur comprenant un oxyde d’yttrium et d’au moins un élément choisi parmi l’hafnium et/ou le titane |
EP4197981A1 (de) | 2021-12-15 | 2023-06-21 | Saint-Gobain Glass France | Verglasung und verfahren zur herstellung davon |
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WO2002062717A1 (en) | 2001-02-08 | 2002-08-15 | Guardian Industries Corp. | Low-e matchable coated articles and methods of making same |
EP0937013B1 (de) | 1997-07-21 | 2002-11-13 | Saint-Gobain Glass France | Durchsichtiges substrat beschichtet mit mindestens einer dünnschicht |
WO2009115596A1 (fr) | 2008-03-20 | 2009-09-24 | Agc Flat Glass Europe Sa | Vitrage revêtu de couches minces |
WO2009157970A1 (en) | 2008-06-25 | 2009-12-30 | Centre Luxembourgeois De Recherches Pour Le Verre Et La Ceramique S.A. (C.R.V.C.) | Coated article with low-e coating including zirconium oxide and/or zirconium silicon oxynitride and methods of making same |
FR2924231B1 (fr) | 2007-11-22 | 2010-05-28 | Saint Gobain | Substrat muni d'un empilement a proprietes thermiques |
WO2011062574A1 (en) | 2009-11-19 | 2011-05-26 | Centre Luxembourgeois De Recherches Pour Le Verre Et La Ceramique S.A. (C.R.V.C.) | Bronze colored coated article with low-e coating |
WO2014191472A2 (en) * | 2013-05-30 | 2014-12-04 | Agc Glass Europe | Low-emissivity glazing |
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US6475626B1 (en) * | 1999-12-06 | 2002-11-05 | Guardian Industries Corp. | Low-E matchable coated articles and methods of making same |
US7166359B2 (en) * | 2005-06-27 | 2007-01-23 | Centre Luxembourgeois De Recherches Pour Le Verre Et La Ceramique S.A. (C.R.V.C.) | Blue colored coated article with low-E coating |
FR2898123B1 (fr) * | 2006-03-06 | 2008-12-05 | Saint Gobain | Substrat muni d'un empilement a proprietes thermiques |
US7655313B2 (en) * | 2007-03-15 | 2010-02-02 | Guardian Industries Corp. | Low-E coated articles and methods of making same |
SG11201506371QA (en) * | 2013-02-14 | 2015-09-29 | Agc Glass Europe | Antisolar glazing |
BR112015022027A2 (pt) * | 2013-03-14 | 2017-07-18 | Agc Glass Europe | vidraça que apresenta uma camada de controle solar |
BR112015029941B1 (pt) * | 2013-05-30 | 2021-12-14 | Agc Glass Europe | Revestimento anti-solar de baixa emissividade |
-
2014
- 2014-12-19 FR FR1462871A patent/FR3030494B1/fr not_active Expired - Fee Related
-
2015
- 2015-12-14 MX MX2017007942A patent/MX2017007942A/es unknown
- 2015-12-14 PL PL15823645T patent/PL3233748T3/pl unknown
- 2015-12-14 ES ES15823645T patent/ES2836351T3/es active Active
- 2015-12-14 KR KR1020177019571A patent/KR102523455B1/ko active IP Right Grant
- 2015-12-14 BR BR112017012191-3A patent/BR112017012191B1/pt active IP Right Grant
- 2015-12-14 WO PCT/FR2015/053473 patent/WO2016097557A1/fr active Application Filing
- 2015-12-14 US US15/536,350 patent/US20170355639A1/en not_active Abandoned
- 2015-12-14 EP EP15823645.5A patent/EP3233748B1/de active Active
-
2017
- 2017-06-13 CO CONC2017/0005826A patent/CO2017005826A2/es unknown
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EP0937013B1 (de) | 1997-07-21 | 2002-11-13 | Saint-Gobain Glass France | Durchsichtiges substrat beschichtet mit mindestens einer dünnschicht |
WO2002062717A1 (en) | 2001-02-08 | 2002-08-15 | Guardian Industries Corp. | Low-e matchable coated articles and methods of making same |
FR2924231B1 (fr) | 2007-11-22 | 2010-05-28 | Saint Gobain | Substrat muni d'un empilement a proprietes thermiques |
WO2009115596A1 (fr) | 2008-03-20 | 2009-09-24 | Agc Flat Glass Europe Sa | Vitrage revêtu de couches minces |
WO2009157970A1 (en) | 2008-06-25 | 2009-12-30 | Centre Luxembourgeois De Recherches Pour Le Verre Et La Ceramique S.A. (C.R.V.C.) | Coated article with low-e coating including zirconium oxide and/or zirconium silicon oxynitride and methods of making same |
WO2011062574A1 (en) | 2009-11-19 | 2011-05-26 | Centre Luxembourgeois De Recherches Pour Le Verre Et La Ceramique S.A. (C.R.V.C.) | Bronze colored coated article with low-e coating |
WO2014191472A2 (en) * | 2013-05-30 | 2014-12-04 | Agc Glass Europe | Low-emissivity glazing |
Also Published As
Publication number | Publication date |
---|---|
BR112017012191A2 (pt) | 2018-01-16 |
PL3233748T3 (pl) | 2021-03-08 |
BR112017012191B1 (pt) | 2022-05-03 |
FR3030494A1 (fr) | 2016-06-24 |
MX2017007942A (es) | 2017-09-15 |
KR102523455B1 (ko) | 2023-04-20 |
KR20170097698A (ko) | 2017-08-28 |
FR3030494B1 (fr) | 2021-09-03 |
WO2016097557A1 (fr) | 2016-06-23 |
CO2017005826A2 (es) | 2017-08-31 |
ES2836351T3 (es) | 2021-06-24 |
US20170355639A1 (en) | 2017-12-14 |
EP3233748A1 (de) | 2017-10-25 |
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